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A Raman Spectroscopic Study of Uranyl Minerals from Cornwall, UK

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A Raman Spectroscopic Study of Uranyl Minerals from Cornwall, UK Electronic Supplementary Material (ESI) for RSC Advances. This journal is © The Royal Society of Chemistry 2014 A Raman spectroscopic study of uranyl minerals from Cornwall, UK R J P Driscoll,a D Wolverson,∗a J M Mitchels,a J M Skelton,a S C Parker,a M Molinari,a I Khan,b D Geeson,b and G C Allenc Received Xth XXXXXXXXXX 20XX, Accepted Xth XXXXXXXXX 20XX First published on the web Xth XXXXXXXXXX 200X DOI: 10.1039/b000000x SUPPORTING INFORMATION a University of Bath, Claverton Down, Bath, UK. ∗ Fax: XX XXXX XXXX; Tel: XX XXXX XXXX; E-mail: [email protected] b AWE, Aldermaston, Reading, UK. c Interface Analysis Center, University of Bristol, Bristol, UK. 1–17 j 1 1 Physical appearance of the uranyl mineral samples Autunite from Merrivale Quarry appears as fine, yellow crystals on a white, grey and black background rock, approximately 6 cm in diameter. Torbernite from Bunny Mine appeared as small (approximately 600 mm across), green, tabular crystals on a grey and brown primary rock, approximately 11 cm in diameter. Nova´cekite˘ from Wheal Edward was present as yellow and green flakes on a black and brown primary rock, approximately 5 cm across. Zeunerite from Wheal Gorland appeared as fine green crystals on a light brown background rock, approx- imately 7 cm across. Phosphuranylite from Wheal Edward occurred as a yellow crust on a brown rock (approximately 7 cm across), with fine, green associated crystals. Andersonite and schrockingerite,¨ both from Geevor Mine, are present as yellow mineral deposits on a brown background rock (both around 4 cm across); both samples have a thin layer of transparent gypsum crystals associated with the uranyl mineral. Johannite from Geevor Mine is present as pale green crystals on a yellow-brown background rock, ap- proximately 5 cm across. Natrozippeite mineral from Geevor Mine occurs as a yellow crust on a black and brown primary rock (about 7 cm across); it is associated with small, green crystals that do not contain a uranyl cation. Uranophane from Wheal Edward is present as a pale yellow crust on a light brown primary rock sample (approximately 7 cm across); it is associated with a black vein of pitchblende. Kasolite from Loe Warren Zawn occurs as an orange-red crust on one face of a large grey primary rock sample, approximately 12 cm across. Compreignacite and cuprosklodowskite were present as dark yellow and green crystals, respectively, on the same sample of brown, black and grey rock from West Wheal Owles. 2 Raman peak tables and wavelength comparisons The tables shown in this section detail the vibrational bands seen in the Raman spectra for each mineral in this investigation. The positions given are an average of the same band seen in multiple spectra of the same sample, and both the standard deviation and the number of spectra in which each peak is seen are given. Literature bands are given; these have typically been deconvoluted. The assignment is based upon that given for the published spectra. The figures shown here illustrate the Raman spectra collected using all three excitation wavelengths for each mineral. 2 j 1–17 Fig. SI 1 A comparison of the three laser wavelengths for the uranyl phosphate mineral autunite. The left figure shows the raw spectra. Each section of the spectra shown on the right have been rescaled, separately, to emphasise the bands. Table SI 1 Raman spectral bands for the uranyl phosphate mineral autunite This Study Literature 2 Position Standard Number Position Attribution (cm−1) Deviation of spectra (cm−1) 193 y 1.7 31 190, 222 Lattice Vibrations 2+ 283 * 4.2 19 291 v2(UO2) bend 3− – – – 399, 406, 439, 464 v2(PO4) bend 3− – – – 629 v4(PO4) bend 2+ 830 3.6 60 816, 822, 833 v1(UO2) symm. stretch 2+ 899 * 4.93 9 – v3(UO2) antisymm. stretch 990 2.67 21 988 3− 1001 x 7.53 31 1007 v3(PO4) symm. stretch 1008 4.16 21 1018 Sixty individual spectra were analysed for this sample of autunite. * Low intensity or broad bands, not always visible in spectra. y The 193 cm−1 peak was most prominent within the 785 nm spectra. x The 1001 cm−1 peak was only visible when the 990 and 1008 cm−1 peaks were not. 1–17 j 3 Fig. SI 2 A comparison of the three laser wavelengths for the uranyl phosphate mineral torbernite. The left figure shows the raw spectra. Each section of the spectra shown on the right have been rescaled, separately, to emphasise the bands. Table SI 2 Raman spectral bands for the uranyl phosphate mineral torbernite This Study Literature 2 Position Standard Number Position Attribution (cm−1) Deviation of spectra (cm−1) 191 * 2.3 26 – Lattice Vibrations 2+ – – – 222, 290 v2(UO2) bend 404 * 2.7 24 399, 406, 439, 464 v (PO )3− bend 440 * 3.9 9 2 4 3− – – – 629 v4(PO4) bend 2+ 825 1.8 38 808, 826 v1(UO2) symm. stretch 2+ 903 * 2.1 10 900 v3(UO2) antisymm. stretch 3− 992 1.75 38 957, 988, 995, 1004 v3(PO4) antisymm. stretch Thirty eight individual spectra were analysed for this sample of torbernite. * Low intensity or broad bands, not always visible in spectra. 4 j 1–17 Fig. SI 3 A comparison of the three laser wavelengths for the uranyl arsenate mineral novacekite. The left figure shows the raw spectra. Each section of the spectra shown on the right have been rescaled, separately, to emphasise the bands. Table SI 3 Raman spectral bands for the uranyl arsenate mineral nova´cekite˘ This Study Literature 10 Literature 2 Position Standard Number Saleeite´ Peak Attribution (cm−1) Deviation of spectra Positions (cm−1) 185 2.9 28 177, 196 – Lattice Vibrations 2+ 269 * 6.0 10 218, 234, 283 284 v2(UO2) bend 3− 325 * 4.3 14 v2(PO4) bend 452 * 2.6 10376, 405, 446, 471 389 or 3− 471 * 5.5 8 v2(AsO4) bend 3− – – – 573, 612 643 v4(PO4) bend 2+ 817 2.6 55 827, 843 818, 833, 847 v1(UO2) symm. stretch 2+ 889 5.6 36 896 – v3(UO2) antisymm. stretch 989 2.3 11 980, 994, 1007 982, 988, 1007 v (PO )3− antisymm. stretch 1034 * 2.6 7 3 4 Fifty five individual spectra were analysed for this sample of nova´cekite.˘ No literature spectra are available for a direct comparison with nova´cekite,˘ so its spectrum has been compared against saleeite,´ its phosphate analogue. * Low intensity or broad bands, not always visible in spectra. 1–17 j 5 Fig. SI 4 A comparison of the three laser wavelengths for the uranyl arsenate mineral zeunerite. The left figure shows the raw spectra. Each section of the spectra shown on the right have been rescaled, separately, to emphasise the bands. Table SI 4 Raman spectral bands for the uranyl arsenate mineral zeunerite This Study Literature 11 Position Standard Number Position Attribution (cm−1) Deviation of spectra (cm−1) – – – 182 Lattice Vibrations 2+ – – – 218, 235, 275 v2(UO2) bend 3− 323 * 4.9 5 320, 380 v2(AsO4) bend 404 * 4.6 7 396 v (AsO )3− bend 463 6.6 19 446, 463 4 4 2+ 821 3.0 25 811, 818 v1(UO2) symm. stretch 2+ 886 4.5 16 890 v3(UO2) antisymm. stretch 987 1.7 9 – unknown 1029 * 2.8 4 – unknown Twenty five individual spectra were analysed for this sample of zeunerite. * Low intensity or broad bands, not always visible in spectra. 6 j 1–17 Fig. SI 5 A comparison of the three laser wavelengths for the uranyl phosphate mineral phosphuranylite. The left figure shows the raw spectra. Each section of the spectra shown on the right have been rescaled, separately, to emphasise the bands. Table SI 5 Raman spectral bands for the uranyl phosphate mineral phosphuranylite This Study Literature 4 Minerva Saddle Ruggles Attribution Position Standard Number Heights Ridge Mine (cm−1) Deviation of spectra Position (cm−1) 148 * 2.3 16 111, 152, 175 117, 145, 166 112, 147, 161 Lattice Vibrations 216 * 4.2 13 211 205 208 239 * 3.7 5 220 227, 240 238 2+ 260 * 3.9 13 263 267 267 v2(UO2) bend 283 * 3.4 5 294 287 295 312 * 5.3 6 3− 435 6.0 25 404, 435, 452 368, 394, 417, 439 396, 398, 421, 437, 452, 476 v2(PO4) bend 3− 558 * 2.7 7 564, 613, 655 500, 532, 566 511, 515, 536, 569, 616 v4(PO4) bend 2+ 801 4.9 29 768, 793, 805, 815 816, 837, 843, 847 812, 817, 832, 841 v1(UO2) symm. stretch 2+ – – – – – 894 v3(UO2) antisymm. stretch 992 y 2.8 10 992 1009 1005 3− 1017 y 1.2 8 1016 1050 1032, 1050, 1055 v3(PO4) antisymm. stretch – – – 1122 1125 1124 Twenty nine individual spectra were analysed for this sample of phosphuranylite. * Low intensity or broad bands, not always visible in spectra. y The 992 and 1017 cm−1 bands appear together, in a small number of 785 nm spectra. 1–17 j 7 Fig. SI 6 A comparison of the three laser wavelengths for the uranyl carbonate mineral andersonite. The left figure shows the raw spectra. Each section of the spectra shown on the right have been rescaled, separately, to emphasise the bands. Table SI 6 Raman spectral bands for the uranyl carbonate mineral andersonite This Study Literature 3 Position Standard Number Position Attribution (cm−1) Deviation of spectra (cm−1) 130 3.1 7 164, 182 Lattice Vibrations 225 * 5.2 8 224, 242, 284, 299 v (UO )2+ bend 291 * 3.3 6 2 2 2− 743 * 2.0 4 697, 732, 744 v4(CO3) bend 2+ 833 0.5 15 830, 833 v1(UO2) symm.
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